The Fertilisers (Sampling and Analysis) Regulations (Northern Ireland) 1991

1Title, commencement and interpretation

2Prescribed amount for the purposes of the definition of sampled portion

3Manner of taking, marking, sealing and fastening up of samples

4Methods of sending part of a sample

5Application of the methods of analysis

6Form of certificate of analysis

7Modification of the Agriculture Act 1970

SCHEDULE 1MANNER OF TAKING, MARKING, SEALING AND FASTENING UP OF SAMPLES

PART IDEFINITIONS

PART IIGENERAL INSTRUCTIONS FOR THE TAKING OF SAMPLES

1In the case of fertiliser in containers, only unopened containers...

2The sample shall be taken and prepared as quickly as...

3A sample shall not be drawn from any part of...

4When stones are naturally present in a fertiliser, they shall,...

5An inspector who intends to take a sample in accordance...

6The sampling apparatus shall be made of materials which cannot...

7In the case of a sampling spear its dimensions shall...

8Notwithstanding the provisions of these Regulations, a sampling spear shall...

9Mechanical apparatus may be used for the sampling of moving...

10Apparatus designed to divide the sample into approximately equal parts...

11A sample taken in accordance with the methods described below...

PART IIIQUANTITATIVE REQUIREMENTS

1Sampled portion

2Incremental sample

3Aggregate sample

PART IVTAKING AND PREPARATION OF SAMPLES

1Incremental samples

2Aggregate sample

3Reduced sample

PART VMARKING, SEALING AND FASTENING UP OF .I-HE FINAL SAMPLE

1Each container of a final sample shall be so secured...

2A label shall be attached to the container or receptacle...

3The container or receptacle may also be sealed, or the...

PART VISAMPLING TABLES

SCHEDULE 2METHODS OF ANALYSIS

2Reagents and Apparatus

3Methods of Analysis

1Preparation of the sample for analysis

2Determination of ammoniacal nitrogen

3(a) Determination of nitrate and ammoniacal nitrogen-Ulsch method

4(a) Determination of nitrogen in calcium cyanamide-in the absence of...

5Determination of total nitrogen in urea

6Determination of cyanamide nitrogen

7Determination of biuret in urea

8(a) Determination of different forms of nitrogen-in the presence of...

9(a) Extraction of total phosphorus-by mineral acids

10Determination of extracted phosphorus

11Determination of water-soluble potassium

12(a) Determination of water-soluble magnesium-atomic absorption spectro-photometric method

13(a) Determination of total magnesium-atomic absorption spectrophoto-metric method

14Determination of chlorides, in the absence of organic matter

15(a) Determination of fineness of grinding—dry method

16Methods of analysis and test procedures for ammonium nitrate fertiliser...

AMethods for the application of thermal cycles

BDetermination of oil retention

CDetermination of the combustible ingredients

DDetermination of the pH value

EDetermination of particle size

FDetermination of the chloride content (as chloride ion)

GDetermination of copper

1.PREPARATION OF THE SAMPLE FOR ANALYSIS

2.1Solid fertilisers: the preparation of a final sample received at...

2.2Fluid fertilisers: the final sample is mixed by shaking to...

3.1Sample divider (optional).

3.2Sieves with apertures of 0.2 mm and 0.5 mm.

3.3250 ml flasks, stoppered.

3.4Porcelain pestle and mortar or grinder.

4CHOICE OF TREATMENT TO BE USED

4.1Final samples which must not be ground

4.2Final samples which must be divided and part of which must be ground

4.3Final samples in respect of which all determinations are carried out on a ground product

7FLUID FERTILISERS

2.DETERMINATION OF AMMONIACAL NITROGEN

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

4.8Sodium hydroxide solution, 30 g per 100 ml ammonia free....

4.9Indicator solutions: Mixed indicator: (4.9.1) Solution A: dissolve 1 g...

4.10Anti-bump granules of pumice stone, washed in hydrochloric acid and...

4.11Ammonium sulphate.

5.1Distillation apparatus consisting of a round-bottomed flask of suitable capacity...

5.2Rotary shaker, 35 to 40 turns per minute.

6PREPARATION OF SAMPLE

7.2Determination

7.4Control test

8EXPRESSION OF THE RESULT

TABLE FOR METHOD 2

3a.DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — ULSCH METHOD

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

4.2Sulphuric acid, 0.1 N solution.

4.3Sodium or potassium hydroxide, 0.1 N solution, carbonate free.

4.4Sulphuric acid solution, approximately 30% H2SO4 (W/V), ammonia free.

4.5Powdered iron reduced in hydrogen. (The prescribed quantity of iron...

4.6Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

4.7Indicator solutions: Mixed indicator: (4.7.1) Solution A: dissolve 1 g...

4.8Anti-bump granules of pumice stone, washed in hydrochloric acid and...

4.9Sodium nitrate.

6PREPARATION OF SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF THE RESULTS

3b.DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — ARND METHOD

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

4.8Sodium hydroxide solution, approximately 2 N.

4.9Arnd’s alloy—powdered so as to pass through a sieve with...

4.1020% Magnesium chloride solution: dissolve 200 g magnesium chloride (MgC12.6H2O)...

4.11Indicator solutions: Mixed indicator: (4.11.1) Solution A: dissolve 1 g...

4.12Anti-bump granules of pumice stone washed in hydrochloric acid and...

4.13Sodium nitrate.

6PREPARATION OF SAMPLE

7.1Preparation of the solution for analysis

7.2Determination

7.4Control test

8EXPRESSION OF THE RESULTS

3c.DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — DEVARDA METHOD

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

4.8Devarda’s alloy—powdered so that 90 to 100% will pass through...

4.9Sodium hydroxide solution, 30 g per 100 ml ammonia free....

4.10Indicator solutions: Mixed indicator: (4.10.1) Solution A: dissolve 1 g...

4.11Ethanol, 95%.

4.12Sodium nitrate.

5.1Distillation apparatus consisting of a round bottomed flask of suitable...

6PREPARATION OF THE SAMPLE

7.1Preparation of the solution for analysis

7.2Determination

7.4Control test

8EXPRESSION OF RESULTS

4aDETERMINATION OF THE TOTAL NITROGEN IN CALCIUM CYANAMlDE — IN THE ABSENCE OF NITRATE

2FIELD OF APPLICATION

4.1Sulphuric acid solution 50% (V/V): dilute an appropriate volume of...

4.2Potassium sulphate.

4.3Copper oxide (CuO) — 0.3 to 0.4 g for each...

4.4Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

4.11Indicator solutions: Mixed indicator: (4.11.1) Solution A: dissolve 1 g...

4.12Anti-bump granules of pumice stone, washed in hydrochloric acid and...

4.13Potassium thiocyanate.

5.1Distillation apparatus. See Method 2.

6PREPARATION OF SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF THE RESULT

4b.DETERMINATION OF TOTAL NITROGEN IN CALCIUM CYANAMIDE — IN THE PRESENCE OF NITRATE

2FIELD OF APPLICATION

4.1Sulphuric acid. (d = 1.84 g/ml).

4.2Powdered iron reduced in hydrogen.

4.3Potassium sulphate, finely pulverised. Sulphuric acid. 0.1 N solution. Sodium or potassium hydroxide, 0.1 N solution, carbonate free. for...

4.10Indicator solutions:

4.11Solution of stannous chloride:

4.12Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

4.13Standard nitrate-ammoniacal solution:

4.14Anti-bump granules of pumice stone, washed in hydrochloric acid and...

6PREPARATION OF THE SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF THE RESULTS

5.DETERMINATION OF TOTAL NITROGEN IN UREA

2FIELD OF APPLICATION

4.1Sulphuric acid, concentrated, (d = 1.84 g/ml).

4.2Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

4.9Indicator solutions:

4.10Anti-bump granules of pumice stone, washed in hydrochloric acid and...

5.1Distillation apparatus. See Method 2.

6PREPARATION OF THE SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF THE RESULT

6.DETERMINATION OF CYANAMIDE NITROGEN

2FIELD OF APPLICATION

4.1Glacial acetic acid.

4.2Ammonia solution: dilute 1 volume of ammonia (d = 0.88...

4.3Ammoniacal silver solution, according to Tollens, freshly prepared: mix 500...

4.4Concentrated sulphuric acid (d = 1.84 g/ml).

4.5Potassium sulphate.

4.6Copper oxide (CuO), 0.3-0.4 g for each determination or an...

4.7Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

4.8Sulphuric acid, 0.1 N solution.

4.9Sodium or potassium hydroxide, 0.1 N solution.

4.10Indicator solutions: Mixed indicator: (4.10.1) Solution A: dissolve 1 g...

4.11Anti-bump granules of pumice stone, washed in hydrochloric acid and...

4.12Potassium thiocyanate.

5.1Distillation apparatus. See Method 2

5.2500 ml graduated flask (for example Stohmann).

5.3Rotary shaker, 35-40 turns per minute.

6PREPARATION OF THE SAMPLE

7.1Safety precaution

7.2Preparation of the solution for analysis

7.3Determination

7.5Control test

8EXPRESSION OF RESULTS

7.DETERMINATION OF BIURET IN UREA

2FIELD OF APPLICATION

4.2Sulphuric acid solution, approximately 0.1 N.

4.3Sodium hydroxide solution, approximately 0.1 N.

4.4Alkaline solution of potassium sodium tartrate: in a 1 litre...

4.5Copper sulphate solution:

4.6Biuret standard solution:

4.7Methyl red indicator solution:

5.1Spectrophotometer.

6PREPARATION OF SAMPLE

7.1Preparation of the standard curve

7.2Preparation of solution for analysis

7.3Determination

8EXPRESSION OF RESULTS

8a.DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME SAMPLE — IN THE PRESENCE OF CYANAMIDE NITROGEN

2FIELD OF APPLICATION

3.1Total soluble and insoluble nitrogen

3.2Forms of soluble nitrogen

4.1Potassium sulphate.

4.2Iron powder, reduced with hydrogen (the prescribed quantity of iron...

4.3Potassium thiocyanate.

4.4Potassium nitrate.

4.5Ammonium sulphate.

4.7Sulphuric acid solution: dilute an appropriate volume of sulphuric acid...

4.8Sulphuric acid, 0.2 N solution.

4.9Sodium hydroxide solution, 30 g per 100 ml. ammonia free....

4.10Sodium or potassium hydroxide, 0.2 N solution, free from carbonates....

4.11Stannous chloride solution: dissolve 120 g of stannous chloride (SnC...

4.12Sulphuric acid, concentrated (d = 1.84 g/ml).

4.13Hydrochloric acid solution: dilute an appropriate volume of hydrochloric acid...

4.14Glacial acetic acid.

4.15Sulphuric acid solution, approximately 30% (W/V) H2SO4.

4.16Ferrous sulphate, crystalline, FeSO4.7H2O.

4.17Sulphuric acid, 0.1 N solution.

4.18Octan-1-o 1.

4.19Potassium carbonate, saturated solution.

4.20Sodium or potassium hydroxide, 0.1 N solution, free from carbonate....

4.21Barium hydroxide, saturated solution.

4.22Sodium carbonate solution, 10 g per 100 ml.

4.23Hydrochloric acid, 2 N solution.

4.24Hydrochloric acid, 0.1 N solution.

4.25Urease solution:

4.26Xanthydrol solution, 5 g per 100 ml in ethanol or...

4.27Copper oxide (CuO): 0.3 to 0.4 g per determination or...

4.28Anti-bump granules washed in hydrochloric acid and ignited.

4.29Indicator solutions: Mixed indicator solution: (4.29.1) Solution A: dissolve 1...

4.30Indicator papers:

4.3Ethanol or methanol: solution 95%.

5.1Distillation apparatus. See Method 2.

5.2Apparatus for the determination of ammoniacal nitrogen according to analytical...

5.3Apparatus for I-tie estimation of urea nitrogen according to the...

5.4Rotary shaker, 35-40 turns per minute.

5.6Laboratory oven.

5.7Sintered glass crucibles, diameter of pores 5 to 15 microns....

6PREPARATION OF THE SAMPLE

7.1Total soluble and insoluble nitrogen

7.2Forms of soluble nitrogen

8VERIFICATION OF THE RESULTS

8.1In certain cases, a difference may be found between the...

8.2Before each analysis, check that the apparatus is working properly...

8b.DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME SAMPLE — IN THE ABSENCE OF CYANAMIDE NITROGEN

2FIELD OF APPLICATION

3.1Total soluble nitrogen

3.2Total soluble nitrogen except nitric nitrogen, by Kjeldahl digestion after...

3.3Nitric nitrogen, by difference: between 3.1.2 and 3.2 and/or between...

3.4Ammoniacal nitrogen, by cold distillation of a weak alkaline solution;...

3.5Urea nitrogen, either: (3.5.1) By conversion using urease, into ammonia,...

4.1Potassium sulphate.

4.2Iron powder, reduced with hydrogen (the prescribed quantity of iron...

4.3Potassium nitrate.

4.4Ammonium sulphate.

4.6Sulphuric acid, 0.2 N solution.

4.7Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

4.8Sodium or potassium hydroxide, 0.2 N solution, free of carbonates....

4.9Sulphuric acid (d = 1.84 g/ml).

4.10Hydrochloric acid solution: dilute an appropriate volume of hydrochloric acid...

4.11Glacial acetic acid.

4.12Sulphuric acid, solution approximately 30% (W/V) H2SO4.

4.13Ferrous sulphate, crystalline FeSO4.7H2O.

4.14Sulphuric acid, 0.1 N solution.

4.15Octal-l-ol.

4.16Potassium carbonate, saturated solution.

4.17Sodium or potassium hydroxide, 0.1 N solution.

4.18Barium hydroxide, saturated solution.

4.19Sodium carbonate solution, 10 g per 100 ml.

4.20Hydrochloric acid, 2 N solution.

4.21Hydrochloric acid, 0.1 N solution.

4.22Urease solution: suspend 0.5 g active unease in 100 ml...

4.23Xanthydrol solution, 5 g per 100 ml in ethanol or...

4.24Catalyst: copper oxide (CuO), 0.3 to 0.4 g per determination,...

4.25Anti-bump granules of pumice stone washed with hydrochloric acid and...

4.26Indicator solutions: Mixed indicator (4.26.1) Solution A: dissolve 1 g...

4.27Indicator papers: litmus, bromothymol blue (or other papers sensitive to...

4.28Ethanol or methanol, 95% (V/V).

5.1Distillation apparatus. See Method 2.

5.2Apparatus for determination of ammoniacal nitrogen. An example of recommended...

5.3Apparatus for determination of urea nitrogen by the urease method...

5.4Rotary shaker: 35 — 40 turns per min.

5.6Sintered glass crucibles, diameter of pores 5 to 15 microns....

6PREPARATION OF SAMPLE

7.1Preparation of solution for analysis

7.2Total nitrogen

7.3Total nitrogen excluding nitric nitrogen

7.4Nitric nitrogen is obtained: by difference between (7.2.4) — (7.5.3...

7.5Ammoniacal nitrogen

7.6Ureic nitrogen

2The titration may also be carried out using an indicator...

8VERIFICATION OF RESULTS

8.1Before each analysis, check the functioning of the apparatus and...

9a.EXTRACTION OF TOTAL PHOSPHORUS BY MINERAL ACIDS

2FIELD OF APPLICATION

4.1Sulphuric acid (d = 1.84 g/ml).

4.2Nitric acid (d = 1.40 g/ml).

5.1A Kjeldahl flask, with a capacity of at least 500...

6PREPARATION OF THE SAMPLE

7.2Determination

9b.EXTRACTION OF PHOSPHORUS BY 2% FORMIC ACID

2FIELD OF APPLICATION

4.1Formic acid, 2% (20 g per litre): dilute 82 ml...

5.1500 ml graduated flask (for example Stohmann).

5.2Rotary shaker, 35 — 40 turns per minute.

6PREPARATION OF THE SAMPLE

7.2Determination

9c.EXTRACTION OF PHOSPHORUS BY 2% CITRIC ACID

2FIELD OF APPLICATION

6PREPARATION OF THE SAMPLE

7.2Determination

9d.EXTRACTION OF PHOSPHORUS BY NEUTRAL AMMONIUM CITRATE

2FIELD OF APPLICATION

4.1Neutral ammonium citrate solution (pH = 7.0). This solution must...

5.2Water bath which can be set thermostatically at 65°C, equipped...

6PREPARATION OF THE SAMPLE

7.2Determination

9e.EXTRACTION OF PHOSPHORUS BY ALKALINE AMMONIUM CITRATE (PETERMANN'S METHOD) AT 65°C

2FIELD OF APPLICATION

4.1Petermann’s solution

Characteristics:

Preparation ,from diammonium citrate:

Preparation from citric acid and ammonia:

Check the ammoniacal nitrogen content as follows:

5.1Water bath which can be maintained at a temperature of...

5.2500 ml graduated flask (for example Stohmann flask).

6PREPARATION OF SAMPLE

7.2Determination

9fEXTRACTION OF PHOSPHORUS BY ALKALINE AMMONIUM CITRATE (PETERMANN'S METHOD) AT AMBIENT TEMPERATURE

2FIELD OF APPLICATION

5.1250 ml graduated flask (for example Stohmann).

5.2Rotary shaker, 35 — 40 turns per minute.

6PREPARATION OF THE SAMPLE

7.2Determination

9g.EXTRACTION OF PHOSPHORUS BY JOULIE'S ALKALINE AMMONIUM CITRATE

2FIELD OF APPLICATION

4.1Joulie’s alkaline solution of ammonium citrate: This solution contains 400...

4.28 — Hydroxyquinoline, (oxine), powdered.

5.1Rotary shaker, 35 — 40 turns per minute.

6PREPARATION OF THE SAMPLE

7.2Determination

9h.EXTRACTION OF PHOSPHORUS BY WATER

2FIELD OF APPLICATION

4.1500 ml graduated flask (for example Stohmann).

4.2Rotary shaker, 35 — 40 turns per minute.

5PREPARATION OF THE SAMPLE

6.2Determination Determine the phosphorus according to Method 10, on an...

10.DETERMINATION OF EXTRACTED PHOSPHORUS

2FIELD OF APPLICATION

4.1Concentrated nitric acid (d = 1.40 g/ml).

4.2Molybdate reagent: Preparation of the reagent based on sodium molybdate:...

5.1Filter crucible with porosity of 5 to 20 microns.

5.2Drying oven regulated at 250°C f 10°C.

5.3Sintered glass funnel with porosity of 5 to 20 microns....

6.1Treatment of the solution

6.2Hydrolysis Bring the contents of the Erlenmeyer flask to the...

6.3Weighing the crucible

6.4Precipitation

6.5Filtering and washing

6.6Drying and weighing

6.8Control test

7EXPRESSION OF THE RESULTS

11.DETERMINATION OF WATER-SOLUBLE POTASSIUM

2FIELD OF APPLICATION

4.1Formaldehyde, 25 — 35% solution, filter if necessary before use....

4.2Potassium chloride.

4.3Sodium hydroxide. 10 N solution. Care should be taken to...

4.4Indicator solution: dissolve 0.5 g phenolphthalein in 100 ml 90%...

4.5EDTA solution: 4 g of the dihydrated disodium salt of...

4.6STPB solution: dissolve 32.5 g sodium tetraphenylborate in 480 ml...

4.7Liquid for washing: dilute 20 ml of the STPB solution...

4.8Bromine water: saturated bromine solution in water.

5.1Filter crucibles with a porosity of 5 to 20 microns....

5.2Oven regulated at 120 ± 10°C.

6PREPARATION OF THE SAMPLE

7.1Extraction Weigh to the nearest 0.001 g, 10 g of...

7.2Determination

7.3Weighing the crucible

7.4Precipitation

7.5Filtering and washing

7.6Drying and weighing

7.8Control test

8EXPRESSION OF RESULTS

8.1Method of calculation and formulae

12a.DETERMINATION OF WATER-SOLUBLE MAGNESIUM — ATOMIC ABSORPTION SPECTROPHOTOMETRlC METHOD

2FIELD OF APPLICATION

4.1Hydrochloric acid, N solution (approximately).

4.2Hydrochloric acid, 0.5 N solution.

4.3Magnesium standard solution: dissolve 1.013 g magnesium sulphate (MgSO4.7H2O) in...

4.4Strontium chloride solution: dissolve 15 g strontium chloride (SrCl2.6H2O) in...

5.1Atomic absorption spectrophotometer with a magnesium lamp (285.2 nm).

6PREPARATION OF SAMPLE

7.2Preparation of the sample solution

7.3Blank solution

7.4Standard solutions for calibration

8EXPRESSION OF THE RESULTS

2b.DETERMINATION OF WATER-SOLUBLE MAGNESIUM —EDTA METHOD

2FIELD OF APPLICATION

4.1Magnesium solution, 0.05 M: weigh out 2.016 g magnesium oxide,...

4.2EDTA solution, 0.05 M: dissolve 18.61 g of the dihydrated...

4.3Calcium solution 0.05 M: weigh out 5.004 g of dry...

4.4Calcein indicator: carefully mix in a mortar 1 ,g calcein...

4.5Calcon carbonic acid indicator: dissolve 400 mg calcon carbonic acid...

4.6Eriochrome black-T indicator: dissolve 300 mg eriochrome black-T in a...

4.7Potassium cyanide solution, 2 g per 100 ml.

4.8Solution of potassium hydroxide and potassium cyanide: dissolve 280 g...

4.9pH 10 buffer solution: dissolve 33 g ammonium chloride in...

5.1Magnetic or mechanical stirrer.

6PREPARATION OF THE SAMPLE

7.2Control test

7.3Determination

8EXPRESSION OF THE RESULTS

13a.DETERMINATION OF TOTAL MAGNESIUM -ATOMIC ABSORPTION SPECTROPHOTOMETRIC METHOD

1SCOPE This method is for the determination of total magnesium....

2FIELD OF APPLICATION

4.1Hydrochloric acid solution 50% (V/V): dilute an appropriate volume of...

4.2Hydrochloric acid, N solution (approximately).

4.3Hydrochloric acid, 0.5 N solution.

4.4Magnesium solution: dissolve 1 ,013 g magnesium sulphate (MgSO4.7H2O) in...

4.5Strontium chloride solution: dissolve 75 g strontium chloride (SrCl2.6H2O) in...

5.1Atomic absorption spectrophotometer with a magnesium lamp (285.2 nm).

6PREPARATION OF SAMPLE

7.2Preparation of the sample solution

7.3Blank solution

7.4Standard solutions for calibration

8EXPRESSION OF THE RESULTS

13b.DETERMINATION OF TOTAL MAGNESIUM —EDTA METHOD

2FIELD OF APPLICATION

4.1Magnesium solution, 0.05 M: weigh out 2.016 g of magnesium...

4.2EDTA solution 0.05 M: dissolve 18.61 g of the dihydrated...

4.3Calcium solution 0.05 M: weigh out 5.004 g of dry...

4.4Calcein indicator: carefully mix in a mortar 1 g of...

4.5Calcon carbonic acid indicator: dissolve 400 mg of calcon carbonic...

4.6Eriochrome black-T indicator: dissolve 300 mg of eriochrome black-T in...

4.7Potassium cyanide solution, 2 g per 100 ml.

4.8Solution of potassium hydroxide and potassium cyanide: dissolve 280 g...

4.9pH 10.5 buffer solution: dissolve 33 g ammonium chloride in...

4.10Hydrochloric acid solution: 50% (V/V): dilute an appropriate volume of...

4.11Sodium hydroxide solution, 5 N.

5.1Magnetic or mechanical stirrer.

6PREPARATION OF THE SAMPLE

7.2Control test

7.3Determination

8EXPRESSION OF THE RESULTS

14.DETERMINATION OF CHLORIDES IN THE ABSENCE OF ORGANIC MATERIAL

2FIELD OF APPLICATION

4.1Nitrobenzene or diethyl ether.

4.2Nitric acid, 10 N solution.

4.3Indicator solution: dissolve 40 g of ferric ammonium sulphate [Fe2(SO4)3.(NH4)2SO4.24H2O]...

4.4Silver nitrate, 0.1 N solution.

4.5Ammonium thiocyanate, 0.1 N solution. Preparation: since this salt is...

5.1Rotary shaker, 35 — 40 turns per minute.

6PREPARATION OF SAMPLE

7.2Determination

7.4Control test

8EXPRESSION OF THE RESULT

15a.DETERMINATION OF FINENESS OF GRINDING — DRY METHOD

2FIELD OF APPLICATION

4.1Mechanical sieve shaker.

4.2Sieves with apertures of 0.160 mm and 0.630 mm respectively...

6EXPRESSION OF THE RESULTS

15b.DETERMINATION OF THE FINENESS OF GRINDING OF SOFT NATURAL PHOSPHATES

2FIELD OF APPLICATION

5.1Sieves with apertures of 0.063 mm and 0.125 mm respectively...

5.2Glass funnel of 20 cm diameter mounted on a stand....

5.3Laboratory oven.

7EXPRESSION OF THE RESULTS

16.METHODS OF ANALYSIS AND TEST PROCEDURES FOR AMMONIUM NITRATE FERTILISERS CONTAINING MORE THAN 28% NITROGEN BY WEIGHT

A.Methods for the Application of Thermal Cycles

1SCOPE AND FIELD OF APPLICATION

2THERMAL CYCLES

2.1Field of application This procedure is for thermal cycling prior...

2.2Principle and definition

B.Determination of Oil Retention

1SCOPE AND FIELD OF APPLICATION

5.1Balance, capable of weighing to the nearest 0.01 gram.

5.2Beakers, of capacity 500 ml.

5.3Funnel, of plastic materials, preferably with a cylindrical wall at...

5.4Test sieve, aperture 0.5 mm, fitting into the funnel (5.3)....

5.6Absorbent tissue (laboratory grade).

6.1Two individual determinations are carried out in quick succession on...

6.3Remove particles smaller than 0.5 mm using the test sieve...

6.3Filter the entire contents of the beaker through the funnel...

6.4Lay two sheets of filter paper (5.5) (about 500 ×...

6.5Repeating the rolling procedure and reweighing

7EXPRESSION OF RESULTS

7.1Method of calculation and formula

C.Determination of the Combustible Ingredients

1SCOPE AND FIELD OF APPLICATION

3.1Analytical-grade chromium VI oxide; Cr-(VI)-03.

3.2Sulphuric acid diluted to 60% by volume: pour 360 ml...

3.3Silver nitrate: 0.1 M solution.

3.4Barium hydroxide: weigh out 15 grams of barium hydroxide (Ba(OH)2.8H2O),...

3.5Hydrochloric acid: 0.1 M standard solution.

3.6Sodium hydroxide: 0.1 M standard solution.

3.7Bromophenol blue: solution of 0.4 grams per litre in water....

3.8Phenolphthalein: solution of 2 grams per litre in 60% by...

3.9Soda lime: particle dimensions, about 1.0 to 1.5 mm.

3.10Demineralised water, freshly boiled to remove carbon dioxide.

4.1Standard laboratory equipment, in particular: filter crucible with a plate...

4.2Compressed nitrogen supply.

4.3Apparatus made up of the following parts and assembled, if...

5.1Sample for analysis

5.2Removal of carbonates

5.3Oxidation and absorption

5.4Measurement of the carbonates originating from organic material

7EXPRESSION OF RESULTS

D.Determination of the pH Value

1SCOPE AND FIELD OF APPLICATION

3.1Buffer solution. pH 6.88 at 20°C

3.2Buffer solution pH 4.00 at 20°C

3.3Commercially available pH standard solutions may be used.

5.1Calibration of the pH meter

5.2Determination

6EXPRESSION OF RESULTS

E.Determination of the Particle Size

1SCOPE AND FIELD OF APPLICATION

3.1200 mm diameter woven-wire test sieves to BS 410 (1986)...

3.2Balance to weigh to 0.1 gram.

3.3Mechanical sieve shaker (if available) capable of imparting both vertical...

4.1The sample is divided representatively into portions of approximately 100...

4.2Weigh one of these portions to the nearest 0.1 gram....

4.3Arrange the nest of sieves in ascending order; receiver 0.5...

4.4Shake by hand or machine, imparting both a vertical and...

4.5Remove the sieves from the nest in turn and collect...

4.6Weigh the material retained on each sieve and that collected...

5EVALUATION OF THE RESULTS

5.1Convert the fraction masses to a percentage of the total...

5.2At least two separate analyses should be carried out and...

6EXPRESSION OF RESULTS

F.Determination of the Chlorine Content (as Chloride Ion)

1SCOPE AND FIELD OF APPLICATION

3.2Concentrated nitric acid (density at 20°C = 1.40 g/ml).

3.3Silver nitrate 0.1 M standard solution. Store this solution in...

3.4Silver nitrate 0.004 M standard solution — prepare this solution...

3.6Potassium chloride, 0.1 M standard reference solution. Weigh, to the...

3.6Potassium chloride, 0.004 M standard reference solution — prepare this...

4.2Bridge, containing a saturated potassium nitrate solution, connected to the...

4.3Magnetic stirrer, with a Teflon-coated rod.

4.4Microburette with fine-pointed tip, graduated in 0.01 ml divisions.

5.1Standardisation of the silver nitrate solution

5.4Determination

6EXPRESSION OF RESULTS

G.Determination of Copper

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid (density at 20°C = 1.18 g/ml).

3.2Hydrochloric acid, 6 M solution.

3.3Hydrochloric acid, 0.5 M solution.

3.4Ammonium nitrate.

3.5Hydrogen peroxide, 30%.

3.6Copper solution (stock): weigh, to the nearest 0.001 gram, 1...

5.1Preparation of the solution for analysis

5.2Blank solution

5.3Determination

6EXPRESSION OF THE RESULTS

2Reagents and Apparatus

3Methods of Analysis

1.Preparation of the sample for analysis

2.Determination of moisture

3.Determination of total nitrogen — chromium powder reduction method

4.Determination of urea

5.aExtraction of phosphorus — by mineral acids (total phosphorus)

bExtraction of phosphorus — by 2% citric acid

6.Determination of extracted phosphorus — spectrophotometric method

7.aDetermination of potassium — gravimetric method

bDetermination of potassium — flame photometric method

8.Determination of total magnesium

9.aDetermination of boron — titrimetric method

bDetermination of boron — spectrophotometric method

10.Determination of cobalt

11.Determination of molybdenum

12.Determination of copper

13.Determination of iron

14.Determination of manganese

15.Determination of the neutralising value in liming materials

16.Determination of fineness of products other than potassic basic slag

17.Determination of fineness of potassic basic stag

1.PREPARATION OF THE SAMPLE FOR ANALYSIS

2SCOPE AND FIELD OF APPLICATION

3.1Solid fertilisers: the whole final sample is ground to the...

3.2Fluid fertilisers: the final sample is thoroughly mixed before each...

4.1Sample grinder capable of grinding the fertiliser to pass the...

4.2Mortar and pestle of suitable material and size.

4.3Sieves having square apertures of 0.18 mm, 0.5 mm and...

4.4Sample containers of non-corrodible materials, with air-tight closures.

5.1Grinding and sieving

5.2Place the prepared sample in a clean container (4.4) and...

5.3Before taking each test portion for analysis, the whole sample...

5.4If the sample contains foreign matter which cannot be ground...

6.1Samples not to be ground

6.2Products which may be difficult to grind mechanically, including products with abnormal moisture or products which become doughy through grinding

6.3Organic materials

6.4Fertilisers comprising several different materials

7FLUID FERTILISERS

2.DETERMINATION OF MOISTURE

1SCOPE AND FIELD OF APPLICATION

3.1Suitable containers with lids ensuring air-tight closure; the dimensions should...

3.2Electricially heated oven, suitably ventilated and capable of being maintained...

4PREPARATION OF SAMPLE

6EXPRESSION OF THE RESULT

3.DETERMINATION OF TOTAL NITROGEN — CHROMIUM POWDER REDUCTION METHOD

1SCOPE AND FIELD OF APPLICATION

3.1Sodium hydroxide solution: 40 g per 100 ml, ammonia free....

3.2Sulphuric acid, 0.1 N solution.

3.3Sulphuric acid, 0.2 N solution.

3.4Sulphuric acid, 0.5 N solution.

3.5Sodium hydroxide, 0.2 N solution, carbonate free.

3.6Chromium metal powder, 100 mesh, low nitrogen content.

3.7Anti-bump granules of pumice stone, washed in hydrochloric acid and...

3.8Anti-foaming agent, paraffin wax.

3.9Sulphuric acid (d = 1.84 g/ml).

3.10Hydrochloric acid (d = 1.18 g/ml).

3.11Catalyst mixture: 1,000 g potassium sulphate and 50 g copper...

3.12Indicator solutions: Mixed indicator: (3.12.1) mix 50 ml of 2...

3.13pH indicator paper, wide range.

5PREPARATION OF SAMPLE

2.0g of the prepared sample, containing not more than 0.06...

6.2Hydrolysis, when the fertiliser is known not to contain organic matter

6.3Digestion, when the fertiliser is known to contain organic matter

6.4Distillation

7EXPRESSION OF THE RESULTS

4.DETERMINATION OF UREA

1SCOPE AND FIELD OF APPLICATION

3.1Activated charcoal.

3.2Carrez solution I: dissolve 21.9 g zinc acetate dihydrate in...

3.3Carrez solution II: 10.6 g potassium ferrocyanide per 100 ml....

3.4Hydrochloric acid solution, 0.02 N.

3.5Sodium acetate solution: 136 g sodium acetate trihydrate per litre....

3.64-dimethylamino-benzaldehyde solution: dissolve 1.6 g of 4-dimethylamino-benzaldehyde (4-DMAB) in 100...

3.7Urea standard solution: 1 .O g per 100 ml (1...

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Determination

6.3Calibration curve

7EXPRESSION OF THE RESULTS

5a.EXTRACTION OF PHOSPHORUS BY MINERAL ACIDS (TOTAL PHOSPHORUS)

1SCOPE AND FIELD OF APPLICATION

3.1Sulphuric acid (d = 1.84 g/ml).

3.2Nitric acid (d = 1.42 g/ml).

4.1A Kjeldahl flask, with a capacity of at least 500...

5PREPARATION OF THE SAMPLE

6.2Determination

5b.EXTRACTION OF PHOSPHORUS BY 2% CITRIC ACID

1SCOPE AND FIELD OF APPLICATION

3.12% citric acid solution (20 g per litre), prepared from...

4.1Rotary shaker: 35 — 40 turns per minute.

5PREPARATION OF THE SAMPLE

6.2Determination

6.DETERMINATION OF EXTRACTED PHOSPHORUS — SPECTROPHOTOMETRIC METHOD

1SCOPE AND FIELD OF APPLICATION

3.1Nitric acid (d =.42 g/ml).

3.2Molybdovanadate reagent: dissolve separately 20 g ammonium molybdate and 0.47...

3.3Phosphorus standard solution: dissolve 4.387 g potassium dihydrogen phosphate, previously...

3.4Sodium hydroxide, approximately 5 N solution.

5.1Determination

6EXPRESSION OF THE RESULTS

7a.DETERMINATION OF POTASSIUM — GRAVIMETRIC METHOD

1SCOPE AND FIELD OF APPLICATION

3.1Formaldehyde, 25 – 35% solution, filtered if necessary before use....

3.2Potassium chloride.

3.3Sodium hydroxide, 10 N solution. Care should be taken to...

3.4Indicator solution: Dissolve 0.5 g phenolphthalein in 100 ml 90%...

3.5EDTA solution: 4 g of the dihydrated disodium salt of...

3.6STPB solution: dissolve 32.5 g sodium tetraphenylborate in 480 ml...

3.7Liquid for washing: dilute 20 ml of the STPB solution...

3.8Hydrochloric acid (d = 1.18 g/ml).

4.1Filter crucibles with a porosity of 5 to 20 microns....

4.2Oven regulated at 120°C + 10°C.

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Determination

6.3Weighing the crucible

6.4Precipitation

6.5Filtering and washing

6.6Drying and weighing

6.8Control test

7EXPRESSION OF THE RESULTS

7b.DETERMINATION OF POTASSIUM — FLAME PHOTOMETRIC METHOD

1SCOPE AND FIELD OF APPLICATION

3.1Ammonia solution (30% V/V): dilute 30 ml concentrated ammonia solution...

3.2Ammonium oxalate solution: saturated aqueous solution.

3.3Hydrochloric acid (d = 1.18 g/ml).

3.4Potassium dihydrogen phosphate: dried for one hour at 105°C.

3.5Potassium solution (stock): dissolve 3.4807 g potassium dihydrogen phosphate (3.4)...

3.6Potassium solution (dilute): dilute 50 ml stock solution (3.5) to...

4.1Flame photometer.

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Blank solution

6.3Determination

7EXPRESSION OF THE RESULTS

8.DETERMINATION OF TOTAL MAGNESIUM

8.1EXTRACTION OF TOTAL MAGNESIUM

1SCOPE AND FIELD OF APPLICATION

1.1This method is applicable to all fertilisers.

2.1Solubilisation by boiling in dilute hydrochloric acid.

3.1Diluted hydrochloric acid: One volume of hydrochloric acid (d =...

4.1Electric hot plate with adjustable temperature.

5PREPARATION OF THE SAMPLE

5.1See Method 1.

6.2Preparation of the solution

8.2DETERMINATION OF MAGNESIUM BY ATOMIC ABSORPTION SPECTROPHOTOMETRY

1SCOPE AND FIELD OF APPLICATION

2.1Determination of magnesium by atomic absorption spectrophotometry after appropriate dilution...

3.1Hydrochloric acid, 1 M solution.

3.2Hydrochloric acid, 0.5 M solution.

3.3Standard solution of magnesium, 1.00 mg/ml. (3.3.1) Dissolve 1.013 grams...

3.4Strontium chloride solution

4.1Spectrophotometer fitted for atomic absorption, with a magnesium lamp, set...

4.2Air-acetylene flame.

5PREPARATION OF THE SAMPLE

5.1See Method 8.1

6.2Preparation of the solution

8.2DETERMINATION OF MAGNESIUM BY ATOMIC ABSORPTION SPECTROPHOTOMETRY

1SCOPE AND FIELD OF APPLICATION

2.1Determination of magnesium by atomic absorption spectrophotometry after appropriate dilution...

3.1Hydrochloric acid, 1 M solution.

3.2Hydrochloric acid, 0.5 M solution.

3.3Standard solution of magnesium, 1.00 mg/ml. (3.3.1) Dissolve 1.013 grams...

3.4Strontium chloride solution

4.1Spectrophotometer fitted for atomic absorption, with a magnesium lamp, set...

4.2Air-acetylene flame.

5PREPARATION OF THE SAMPLE

5.1See Method 8.1

6.1If the fertiliser has a declared magnesium (Mg) content of...

6.2Using a pipette, take 10 ml of the extraction solution...

6.3Dilute this solution (6.2) with the 0.5 M hydrochloric acid...

6.4Preparation of blank solution

6.5Preparation of calibration solutions

7EXPRESSION OF RESULTS

9a.DETERMINATION OF BORON — TITRIMETRIC METHOD

1SCOPE AND FIELD OF APPLICATION

3.1Calcium oxide.

3.3Sodium carbonate.

3.4Hydrochloric acid solution 50% (V/V): dilute 50 ml concentrated hydrochloric...

3.5Hydrochloric acid, 0.5 N solution.

3.6Lead nitrate solution, 10 g per 100 ml.

3.7Sodium hydroxide, 0.5 N solution.

3.8Sodium hydroxide, 0.05 N solution, carbonate free.

3.9Methyl red indicator solution: dissolve 0.1 g of methyl red...

3.10Phenolphthalein indicator solution: dissolve 0.25 g phenolphthalein in 1.50 ml...

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Determination

7EXPRESSION OF THE RESULT

9b.DETERMINATION OF BORON — SPECTROPHOTOMETRIC METHOD

1SCOPE AND FIELD OF APPLICATION

3.1Calcium oxide.

3.2Sulphuric acid (d = 1.84 g/ml).

3.3Carminic acid solution: dissolve 0.025 g carminic acid in sulphuric...

3.4Hydrochloric acid solution 20% (V/V): dilute 20 ml hydrochloric acid...

3.6Hydrazine hydrate (approximately 60% W/W solution).

4.1Spectrophotometer with 10 mm cells.

5PREPARATION OF THE SAMPLE

6.1Preparation of the solution for analysis

6.3Determination

6.4Calibration curve

7EXPRESSION OF THE RESULTS

10.DETERMINATION OF COBALT

1SCOPE AND FIELD OF APPLICATION

3.1Sodium sulphate, anhydrous.

3.3Hydrochloric acid, 2 N solution.

3.4Hydrochloric acid solution, 50% (V/V): dilute 50 ml concentrated hydrochloric...

3.5Hydrogen peroxide solution, 3% (10 volume).

3.6Nitric acid solution, 30% (V/V): dilute 30 ml nitric acid...

3.72-nitroso-I-naphthol solution: dissolve 1 g of 2-nitroso-1-naphthol in 100 ml...

3.8Sodium citrate solution: 40 g per 100 ml.

3.9Sodium hydroxide, 2 N solution.

3.10Cobalt solution (stock): weigh to the nearest 0.001 g, 0.670...

3.11Cobalt solution (working standard): dilute the stock cobalt solution (3.10)...

4.1Spectrophotometer with 10 mm cells.

5PREPARATION OF THE SAMPLE

6.1Preparation of the solution for analysis

6.2Determination

6.3Calibration Curve

7EXPRESSION OF THE RESULTS

11.DETERMINATION OF MOLYBDENUM

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid, 50% (V/V): dilute 50 ml concentrated hydrochloric acid...

3.2Hydrochloric acid, 2 N solution.

3.3Hydrochloric acid, N solution.

3.4Nitric acid solution, 30% (V/V): dilute 30 ml nitric acid...

3.6Ammonium ferrous sulphate solution, 4 g per 100 ml.

3.7Potassium thiocyanate solution, 40 g per 100 ml.

3.8Sodium sulphate, anhydrous.

3.9Stannous chloride solution: suspend 40 g stannous chloride dihydrate in...

3.10Solvent mixture: mix equal volumes of carbon tetrachloride and 3-methylbutan-1-01....

4.1Spectrophotometer with 10 mm cells.

5PREPARATION OF THE SAMPLE

6.1,Preparation of the solution for analysis

6.2Determination

7EXPRESSION OF THE RESULTS

12.DETERMINATION OF COPPER

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid (d = 1.18 g/ml).

3.2Hydrochloric acid, 6 N solution.

3.3Hydrochloric acid, 0.5 N solution.

3.4Hydrogen peroxide, approximately 100 volume, 30% by weight. Copper solution...

4.1Atomic absorption spectrophotometer with a copper lamp (324.8 nm).

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Blank Solution

6.3Determination

7EXPRESSION OF THE RESULTS

13.DETERMINATION OF IRON

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid (d = 1.18 g/ml).

3.2Hydrochloric acid, 6 N solution.

3.3Hydrochloric acid, 0.5 N solution.

3.4Hydrogen peroxide, approximately 100 volume, 30% by weight.

3.6Lanthanum chloride solution: dissolve 12 g lanthanum oxide in 150...

4.1Atomic absorption spectrophotometer with an iron lamp (248.3 nm).

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Blank solution

6.3Determination

7EXPRESSION OF THE RESULTS

14.DETERMINATION OF MANGANESE

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid (d = 1.18 g/ml).

3.2Hydrochloric acid, 6 N solution.

3.3Hydrochloric acid, 0.5 N solution. Manganese solution (stock):

3.5Lanthanum chloride solution: dissolve 12 g lanthanum oxide in 150...

4.1Atomic absorption spectrophotometer with a manganese lamp (279.5 nm).

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Blank solution

6.3Determination

7EXPRESSION OF THE RESULTS

15.DETERMINATION OF THE NEUTRALISING VALUE IN LIMING MATERIALS

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid, 0.5 N solution.

3.2Sodium hydroxide, 0.5 N solution of carbonate free).

3.3Phenolphthalein indicator solution: dissolve 0.25 g phenolphthalein in 150 ml...

4PREPARATION OF SAMPLE

5.1Determination

6EXPRESSION OF THE RESULTS

16.DETERMINATION OF FINENESS OF PRODUCTS OTHER THAN POTASSIC BASIC SLAG

1SCOPE AND FIELD OF APPLICATION

4.1For sieving through 3.55 mm, 1.0 mm and 150 micron sieves

4.2For sieving through 6.7 mm, 6.3 mm and 5 mm sieves

4.3For sieving through a 45 mm sieve

5EXPRESSION OF THE RESULTS

17.DETERMINATION OF FINENESS OF POTASSIC BASIC SLAG

1SCOPE AND FIELD OF APPLICATION

4.1Preparation of the sample

5EXPRESSION OF THE RESULTS

APPENDIX TO SCHEDULE 2

KEY TO FIGURE 1

KEY TO FIGURE 2

KEY TO FIGURE 3

KEY TO FIGURE 4

KEY TO FIGURE 5

KEY TO FIGURE 6

KEY TO FIGURE 7

KEY TO FIGURE 8

1991 No. 540

AGRICULTURE

The Fertilisers (Sampling and Analysis) Regulations (Northern Ireland) 1991

Made19th December 1991

Coming into operation17th February 1992

The Department of Agriculture in exercise of the powers conferred on it by sections 66(1), 74A, 75(1), 76(1), 77, 78(2), (4) and (6), 79(1), (2) and (9), 84 and 86(1), (2), (3) and (9) of the Agriculture Act 19701 and of all other powers enabling it in that behalf, after consultations with such persons or organisations as appear to it to represent the interests concerned, hereby makes the following Regulations:—